CN115318210B - Preparation method and application of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding - Google Patents
Preparation method and application of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 67
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 62
- 239000004964 aerogel Substances 0.000 title claims abstract description 51
- XUKVMZJGMBEQDE-UHFFFAOYSA-N [Co](=S)=S Chemical compound [Co](=S)=S XUKVMZJGMBEQDE-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 14
- 239000010941 cobalt Substances 0.000 claims abstract description 14
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 239000003921 oil Substances 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 239000011358 absorbing material Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 229940011182 cobalt acetate Drugs 0.000 claims description 3
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 3
- PFQLIVQUKOIJJD-UHFFFAOYSA-L cobalt(ii) formate Chemical compound [Co+2].[O-]C=O.[O-]C=O PFQLIVQUKOIJJD-UHFFFAOYSA-L 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 2
- 239000005715 Fructose Substances 0.000 claims description 2
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- ZZYSOUTXXFZJBK-UHFFFAOYSA-L butanoate;cobalt(2+) Chemical compound [Co+2].CCCC([O-])=O.CCCC([O-])=O ZZYSOUTXXFZJBK-UHFFFAOYSA-L 0.000 claims description 2
- TZWGXFOSKIHUPW-UHFFFAOYSA-L cobalt(2+);propanoate Chemical compound [Co+2].CCC([O-])=O.CCC([O-])=O TZWGXFOSKIHUPW-UHFFFAOYSA-L 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 125000000185 sucrose group Chemical group 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 23
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 4
- 239000007833 carbon precursor Substances 0.000 description 4
- 150000001868 cobalt Chemical class 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- -1 transition metal disulfide Chemical class 0.000 description 3
- 239000004966 Carbon aerogel Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002057 nanoflower Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
- B01J27/224—Silicon carbide
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Dispersion Chemistry (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A preparation method and application of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding relate to the technical field of wave-absorbing and electromagnetic shielding material preparation. The invention aims to solve the existing CoS 2 The preparation of the composite material has the problems of poor thermal stability, multiple steps, low yield and the like, and expands CoS 2 The application of the composite material in the aspect of absorbing electromagnetic waves. The method comprises the following steps: dissolving an organic cobalt source and a carbon source in water, and mixing to form a solution I; dissolving sulfur powder into white oil to obtain a solution II; adding silicon carbide into a surfactant solution to obtain a solution III; mixing the solutions I, II and III, performing hydrothermal reaction, and centrifuging and filtering to obtain CoS 2 Annealing the porous carbon/SiC precursor to obtain CoS 2 Porous carbon/SiC aerogel composite. The invention has the advantages of environment friendliness, easily available reagents, simple equipment and easy operation, and is suitable for popularization.
Description
Technical Field
The invention relates to the field of electromagnetic shielding and wave absorbing material preparation, in particular to a preparation method and application of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding.
Background
With the rapid development of national defense construction, electronic information and communication technology, the influence of electromagnetic radiation on human health and natural environment is reduced, more invisible equipment is produced, and the like, the modern wave-absorbing materials with thin, light, wide and strong properties are required to be developed. The material has the characteristics of good electric performance and magnetic performance, light weight and stability, and the development of light weight and high efficiency wave absorbing materials becomes a hot problem in technological research and development.
CoS 2 Is pyrite type transition metal disulfide with excellent performance, and has stronger magnetism because a 3d electronic layer is not filled. Relative NiS 2 、FeS 2 The semiconductor material has excellent electrochemical performance, high conductivity, small internal resistance, strong loading capacity and the like, and is applied to the aspects of catalysts, magnetic materials, photosensitive materials and high-energy-density battery materials.
CoS 2 Is difficult to exist alone in nature, and is synthesized by adopting a manual method (J Mater Chem A, 2013:5741-5746) by using Co (NO 3 ) 2 ·6H 2 O is cobalt source, CS 2 CoS is prepared by hydrothermal method as sulfur source 2 And (3) powder. (J Mater Chem A, 2013:5741-5746), but CoS prepared 2 The purity is lower, and CoS impurities are contained. In patent 1 (CN 111403180B), carbon cloth is placed in a mixed solution of imidazole organic ligand and cobalt salt, and is kept stand for 4 to 6 hours, and then the carbon cloth is placed in an alcohol solution of a sulfur source for heating treatment, so that cobalt disulfide nanorods are generated on the surface of the carbon cloth. And then nickel hydroxide is deposited on the surface of the nano rod and is applied to the flexible super capacitor. Patent 2 (CN 112563471B) is a preparation method of cobalt disulfide/carbon hollow nanoflower composite material, which is to drop ethyl orthosilicate into water and absolute ethyl alcohol to obtain silica nanospheres; mixing and heating silica spheres with urea and cobalt salt; adding the product into a mixture of dopamine and tris (hydroxymethyl) aminomethane to obtain a polydopamine-coated cobalt silicate/silicon dioxide composite material; and then placing the material in a tubular furnace and performing heat treatment in a protective atmosphere to obtain a precursor, performing heat treatment on the precursor in the protective atmosphere, performing heat treatment, then placing the material in hydrofluoric acid for etching, and finally obtaining the cobalt disulfide/carbon hollow nanoflower composite material. The sodium ion battery anode material has excellent cycle stability and rate capability. However, the process has more operation steps, more complex process and lower yield.
To sum up, coS 2 The preparation methods of the composite material are numerous, but the preparation methods have the defects of complex process, low purity of finished products, poor thermal stability and the like, and CoS 2 Although the material has good magnetic and electrochemical properties, the material is often used as a positive electrode material of a thermal battery and a negative electrode material of a sodium ion battery, and is applied to electromagnetic shielding and wave absorbing materials, which is rarely reported.
Disclosure of Invention
The invention provides a preparation method and application of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding. Silicon carbide with high hardness and adjustable resistivity is used as a framework material, so that the thermal stability of the material is improved; the unique characteristics of ultralow density and high porosity of the aerogel reduce the quality. The high porosity of the porous carbon increases the specific surface area, is favorable for generating strong multiple scattering loss of electromagnetic waves in the material, improves the absorption performance of aerogel, and reduces the cost. Thereby achieving the purpose of preparing stable, light and high-efficiency cobalt disulfide wave-absorbing composite materials.
The preparation method of the cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding is carried out according to the following steps:
respectively dissolving an organic cobalt source and a carbon source in water, and mixing to form a solution I;
step two, dissolving sulfur powder into white oil to obtain a solution II;
adding silicon carbide particles into a surfactant solution with the mass percentage of 0.01% -1%, and magnetically stirring for 10-30 min to obtain a solution III;
step four, mixing the solutions I, II and III under magnetic stirring to obtain a solution IV; transferring the solution IV into a reaction kettle, performing hydrothermal reaction, and naturally cooling the product to room temperature;
step five, opening the reaction kettle, discarding supernatant, and taking down the solid; centrifuging the lower layer solid, washing with distilled water, glycol and HCl solution to obtain black precipitate CoS 2 Porous carbon/SiC precursor;
step six, coS is carried out 2 Mixing porous carbon/SiC precursor with sulfur powder, and annealing in protective atmosphere to obtain CoS with polygonal sheet structure 2 Porous carbon/SiC aerogel composite.
Further, the organic cobalt source in the first step is cobalt formate, cobalt acetate, cobalt propionate or cobalt butyrate; the carbon source is sucrose, glucose or fructose; the mass ratio of the organic cobalt source to the carbon source is 0.5-10: 2 to 25.
Further, the mass fraction of the sulfur powder in the solution II in the second step is 1-30%; solution II was prepared as follows: stirring for 10-40 min at 20-60 ℃ and rotating speed of 100-400 r/min.
Further, in the fourth step, the mixing volume ratio of the solutions I, II and III is 1-25: 1-20: 0.01 to 10; firstly, dropwise adding the solution II into the solution I, stirring for 10-30 min at room temperature and a rotating speed of 100-400 r/min, adding the solution III, and stirring for 20-50 min at a rotating speed of 200-500 r/min to obtain a reaction solution IV.
Further, the hydrothermal reaction temperature in the step four is 120-260 ℃ and the reaction time is 10-24 hours.
Further, the speed of centrifugation in the fifth step is 3000 r/min-8000 r/min, and the centrifugation time is 5 min-15 min.
Further, in the fifth step, distilled water, ethanol and HCl solution are alternately washed, wherein the concentration of the HCl solution is 0.2-3 mol/L.
Further, the annealing treatment temperature in the step six is 400-900 ℃, the heating speed is 0.5-5 ℃/nim, and the constant temperature time is 1-5 h.
Further, the CoS of the manufactured polygonal sheet structure 2 The porous carbon/SiC aerogel composite material is of a polygonal sheet structure, the particle size is 10-100nm, wherein cobalt disulfide is used as a shell, and silicon carbide is used as a core.
The cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding is used as an electromagnetic shielding and wave absorbing material.
The invention has the following beneficial technical effects:
(1) The invention relates to a preparation method of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding, which takes organic cobalt source and sulfur powder as raw materials and prepares the composite material through a hydrothermal method and annealing, heating and drying (or freeze drying). The obtained product has high purity, and the size of the cobalt sulfide microsphere can be regulated and controlled by changing the reaction temperature and time.
(2)CoS 2 Low resistance, good conductivity and magnetism, increased dielectric loss and magnetic loss, and more electromagnetic waves are dissipated in an energy form, so that the wave absorbing performance of the material is improved.
(3)(SiC) P Is a ceramic material with excellent performance, and the resistivity is 10 -2 ～10 6 The material has the advantages of being continuous and adjustable along with the change of the manufacturing process, being an ideal framework material and increasing the thermal stability of the finished product.
(4) The specific porous structure of the porous carbon and the aerogel can reduce CS 2 The self-agglomeration of the aerogel increases the stability of the material, can reduce the obstruction of electromagnetic waves entering the aerogel, and eliminates the influence of impedance mismatch; meanwhile, a richer surface is provided, so that trapped electromagnetic waves are internally reflected and scattered for multiple times, and energy consumption is realized, so that the composite material has good electromagnetic shielding property, and is beneficial to electromagnetic wave absorption and application in the electrochemical field.
(5) The aerogel is light, can reduce the weight of the wave-absorbing material, and reaches the characteristic requirement of light weight.
(6) The method is environment-friendly, simple to operate, easy to obtain raw materials, low in equipment requirement, free of adjusting the pH value of the solution and adding morphology control agents, and suitable for popularization and application.
(7) The finished product of the invention has high purity. Soluble cobalt salt remains and CoS byproducts are often generated in the hydrothermal reaction process, and unreacted soluble cobalt salt is removed by distilled water in the patent; coS is removed by a certain concentration of non-oxidizing acid-HCl, so that CoS is improved 2 Product purity.
(8) The invention has multiple loss mechanisms such as interface loss, polarization loss, dielectric loss, magnetic loss and the like, can realize broadband loss with the microwave band (2-18 GHz band) higher than 90 percent, and has high-efficiency and light wave absorbing characteristics. The invention is mainly applied to the fields of electromagnetic shielding and wave absorption, and can be also applied to electrode material preparation, catalytic materials, photoelectric materials and the like.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is an XRD spectrum of "cobalt disulfide/porous carbon/silicon carbide aerogel" prepared in example 1 of the present invention;
FIG. 2 is an SEM photograph of "cobalt disulfide/porous carbon/silicon carbide aerogel" prepared in example 1 of the present invention;
FIG. 3 is a TEM photograph of "cobalt disulfide/porous carbon/silicon carbide aerogel" prepared in example 1 of the present invention;
FIG. 4 is a graph showing the wave absorption curve of "cobalt disulfide/porous carbon/silicon carbide aerogel" prepared in example 1 of the present invention.
In the figure, A has a thickness of 1mm, B has a thickness of 1.5mm, C has a thickness of 2mm, D has a thickness of 2.5mm, E has a thickness of 3mm, F has a thickness of 4mm, G has a thickness of 3.5mm, H has a thickness of 4.5mm, and I has a thickness of 5mm.
Detailed Description
For the purposes of clarity, technical solutions and advantages of embodiments of the present invention, the spirit of the present disclosure will be described in detail below, and any person skilled in the art, after having appreciated the embodiments of the present disclosure, may make changes and modifications to the techniques taught by the present disclosure without departing from the spirit and scope of the present disclosure.
The exemplary embodiments of the present invention and the descriptions thereof are intended to illustrate the present invention, but not to limit the present invention.
Examples
The preparation method of the cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding in the embodiment comprises the following steps:
example 1
Respectively dissolving 2g of cobalt acetate and 5g of sucrose in 100ml of water, and mixing to form a solution I;
dissolving 4g of sulfur powder into 50ml of white oil, magnetically stirring for 30min at 50 ℃ and rotating at 300r/min to form a solution II;
and thirdly, adding 4g of silicon carbide particles into 400ml of 0.05% surfactant solution, and magnetically stirring for 10-30 min to obtain solution III.
Step four, under magnetic stirring, dropwise adding 40ml of solution II into 30ml of solution I, stirring for 20min at room temperature at a rotating speed of 300r/min, adding 10ml of solution III, stirring for 30min at a rotating speed of 400r/min, and obtaining a reaction solution IV; transferring the solution III into a polytetrafluoroethylene reaction kettle, heating the solution III in an oven to 200 ℃, performing hydrothermal reaction for 18 hours, and naturally cooling the product to room temperature.
And fifthly, opening the reaction kettle, discarding supernatant, and taking down the solid. And (3) centrifugally filtering the lower layer solid, and washing the lower layer solid with distilled water, glycol and HCl solution for 2 times respectively, wherein the concentration of the HCl solution is 1.5mol/L, the centrifugal speed is 5000r/min, and the centrifugal time is 7min. Obtain black precipitated CoS 2 Porous carbon precursor.
Step six, coS is carried out 2 Mixing porous carbon precursor with sulfur powder, annealing at 700 deg.C and 1 deg.C/nim under protective atmosphere, and maintaining the temperature for 2 hr to obtain core-shell CoS 2 Porous carbon/silicon carbide aerogel. Cobalt disulfide is used as a shell layer, and silicon carbide is used as a core.
Test method
Observing the microscopic morphology of cobalt disulfide/porous carbon/silicon carbide aerogel by using a VEGA3 XMU scanning electron microscope; analyzing the phase of cobalt disulfide/porous carbon/silicon carbide aerogel by using an Shimadzu XRD-6100 type X-ray diffractometer; the dielectric property of the sample is tested by adopting an HP8722ES type vector network analyzer, and the testing method is a waveguide method. Mixing the particles to be tested with paraffin according to the proportion of 2:3 are uniformly mixed in proportion, and are pressed into a circular ring with the inner diameter of 3.0mm, the outer diameter of 7.0mm and the thickness of 2.0 mm. Its electromagnetic parameters were tested in the 2-18GHz range and analyzed by Matlab fitting, etc.
Test results
FIG. 1 is an XRD diffraction peak of cobalt disulfide/porous carbon/silicon carbide aerogel composite. As can be seen from FIG. 1, the XRD diffraction peaks of cobalt disulfide/porous carbon/silicon carbide aerogel are compared with CoS 2 The diffraction peaks given by the standard card JCDF No. 41-1471 are better matched, illustrating CoS 2 Well supported on the porous carbon aerogel framework.
FIG. 2 is an SEM of a cobalt disulfide/porous carbon/silicon carbide aerogel composite at high and low magnification. FIG. 2 (a) shows SEM at low magnification, and it can be seen that cobalt disulfide/porous carbon/silicon carbide has a polygonal plate structure of about 20-100nm in diameter, and the polygonal plate structure has uniform particle size and is stacked on each other. FIG. 2 (b) is a high magnification SEM, where the morphology of the individual cobalt disulfide/porous carbon/silicon carbide aerogel composite can be clearly seen; the cobalt disulfide composite material with the polygonal sheet structure has larger specific surface area, is favorable for repeated reflection and refraction of electromagnetic waves, and enhances the wave absorbing performance of the material.
Fig. 3 is a TEM photograph of a cobalt disulfide/porous carbon/silicon carbide aerogel composite. The internal structure of the stacked layers of multilateral sheets can be seen more clearly from fig. 3.
FIG. 4 is a graph of the wave absorption curve of a cobalt disulfide/porous carbon/silicon carbide aerogel composite. As can be seen from FIG. 4, all R of the material are in the range of 1.0-5.0mm in thickness at a frequency of 2-18GHz L The values are smaller than-10 d B, which indicates that the cobalt disulfide/porous carbon/silicon carbide aerogel has strong electromagnetic wave absorption capacity as a whole. In particular, when the sample thickness is 2.5mm and the frequency is 9.84GHz, R is R L Values up to-42.21 d B; when the thickness of the sample is 5.0mm and the frequency is 14.16GHz, R is R L The value reaches-46.7963 dB, which means that the electromagnetic wave energy incident to the surface of the material has more than 99.9 percent of absorbed loss, thus indicating that the cobalt disulfide/porous carbon/silicon carbide aerogel has good wave absorbing performance.
Example 2
Respectively dissolving 2g of cobalt formate and 4g of glucose in 100ml of water, and mixing to form a solution I;
dissolving 3g of sulfur powder into 40ml of white oil, magnetically stirring at 40 ℃ for 20min, and rotating at 200r/min to form a solution II;
and thirdly, adding 2g of silicon carbide particles into 250ml of 0.1% surfactant solution, and magnetically stirring for 20min to obtain a solution III.
Step four, under magnetic stirring, dropwise adding 35ml of solution II into 28ml of solution I, stirring for 20min at room temperature at a rotating speed of 300r/min, adding 8ml of solution III, stirring for 30min at a rotating speed of 300r/min, and obtaining a reaction solution IV; transferring the solution III into a polytetrafluoroethylene reaction kettle, heating the solution III in an oven to 200 ℃, performing hydrothermal reaction for 15 hours, and naturally cooling the product to room temperature.
And fifthly, opening the reaction kettle, discarding supernatant, and taking down the solid. And (3) centrifugally filtering the lower layer solid, and washing the lower layer solid for 2 times by using distilled water, glycol and HCl solution respectively, wherein the concentration of the HCl solution is 1.0mol/L, the centrifugal speed is 5000r/min, and the centrifugal time is 5min. Obtain black precipitated CoS 2 Porous carbon precursor.
Step six, coS is carried out 2 Mixing porous carbon precursor with sulfur powder, annealing at 600deg.C at a heating rate of 1deg.C/nim under protective atmosphere, and maintaining the temperature for 2 hr to obtain core-shell CoS 2 Porous carbon aerogel. Cobalt disulfide is used as a shell layer, and porous carbon is used as a core.
Test method
Observing the microscopic morphology of cobalt disulfide/porous carbon/silicon carbide aerogel by using a VEGA3 XMU scanning electron microscope; qualitative analysis of the phase of cobalt disulfide/porous carbon/silicon carbide aerogel by using an Shimadzu XRD-6100 type X-ray diffractometer; the dielectric property of the sample is tested by adopting an HP8722ES type vector network analyzer, and the testing method is a waveguide method. Mixing the particles to be tested with paraffin according to the proportion of 2:3 are uniformly mixed in proportion, and are pressed into a circular ring with the inner diameter of 3.0mm, the outer diameter of 7.0mm and the thickness of 2.0 mm. Its electromagnetic parameters were tested in the 2-18GHz range and analyzed by Matlab fitting, etc.
Test results
XRD diffraction peak and CoS of cobalt disulfide/porous carbon/silicon carbide aerogel 2 The diffraction peaks given by the standard card JCPDF No41-1471 are better matched and exhibit the same effect as in fig. 1. SEM showed similar effect to fig. 2, cobalt disulfide/porous carbon/silicon carbide was a polygonal sheet structure with uniform particle size, stacked on top of each other. As can be seen from the wave absorption curve of cobalt disulfide/porous carbon/silicon carbide aerogel, all R of the material are in the range of 2-18GHz in frequency and 1.0-5.0mm in thickness L The values are smaller than-10 dB, which indicates that the cobalt disulfide/porous carbon/silicon carbide aerogel has strong electromagnetic wave absorption capacity as a whole. In particular, when the sample thickness is 3.0mm and the frequency is 10.32GHz, R is R L Values of-39.47 d B can be achieved; when the thickness of the sample is 5.0mm and the frequency is 13.74GHz, R is R L The value reaches-41.62 dB, and the value reaches-41.62 dB,meaning that electromagnetic wave energy incident on the surface of the material will have more than 99.9% absorbed loss, indicating that cobalt disulfide/porous carbon/silicon carbide aerogel has good wave absorbing properties.
The above embodiments are merely exemplary descriptions of the present invention, and it should be noted that any simple variations, modifications or other equivalent alternatives which do not take the inventive effort by a person skilled in the art can fall within the scope of protection of the present invention without departing from the core of the present invention.
Claims (10)
1. The preparation method of the cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding is characterized by comprising the following steps of:
respectively dissolving an organic cobalt source and a carbon source in water, and mixing to form a solution I;
step two, dissolving sulfur powder into white oil to obtain a solution II;
adding silicon carbide particles into a surfactant solution with the mass percentage of 0.01% -1%, and magnetically stirring for 10-30 min to obtain a solution III;
step four, mixing the solutions I, II and III under magnetic stirring to obtain a solution IV; transferring the solution IV into a reaction kettle, performing hydrothermal reaction, and naturally cooling the product to room temperature;
step five, opening the reaction kettle, discarding supernatant, and taking down the solid; centrifuging the lower layer solid, washing with distilled water, glycol and HCl solution to obtain black precipitate CoS 2 Porous carbon/SiC precursor;
step six, coS is carried out 2 Mixing porous carbon/SiC precursor with sulfur powder, and annealing in protective atmosphere to obtain CoS with polygonal sheet structure 2 Porous carbon/SiC aerogel composite.
2. The method for preparing cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding according to claim 1, wherein the organic cobalt source in the first step is cobalt formate, cobalt acetate, cobalt propionate or cobalt butyrate; the carbon source is sucrose, glucose or fructose; the mass ratio of the organic cobalt source to the carbon source is 0.5-10: 2 to 25.
3. The method for preparing cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding according to claim 1, wherein the mass fraction of sulfur powder in the solution II in the second step is 1% -30%; solution II was prepared as follows: stirring for 10-40 min at 20-60 ℃ and rotating speed of 100-400 r/min.
4. The method for preparing cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding according to claim 1, wherein the volume ratio of the mixed solutions I, II and III in the fourth step is 1-25: 1-20: 0.01 to 10; firstly, dropwise adding the solution II into the solution I, stirring for 10-30 min at room temperature and a rotating speed of 100-400 r/min, adding the solution III, and stirring for 20-50 min at a rotating speed of 200-500 r/min to obtain a reaction solution IV.
5. The method for preparing cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding according to claim 1, wherein the hydrothermal reaction temperature in the fourth step is 120-260 ℃ and the reaction time is 10-24 h.
6. The method for preparing cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding according to claim 1, wherein the centrifugation speed in the fifth step is 3000 r/min-8000 r/min, and the centrifugation time is 5 min-15 min.
7. The method for preparing cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding according to claim 1, wherein distilled water, ethylene glycol and HCl solution are alternately washed in the fifth step, wherein the concentration of the HCl solution is 0.2-3 mol/L.
8. The method for preparing cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding according to claim 1, wherein the annealing treatment temperature in the step six is 400-900 ℃, the heating rate is 0.5-5 ℃/nim, and the constant temperature time is 1-5 h.
9. The method for preparing cobalt disulfide/porous carbon/silicon carbide aerogel composite for electromagnetic shielding according to claim 1, wherein the prepared CoS with polygonal lamellar structure is characterized in that 2 The porous carbon/SiC aerogel composite material is of a polygonal sheet structure, the particle size is 10-100nm, wherein cobalt disulfide is used as a shell, and silicon carbide is used as a core.
10. The use of a cobalt disulfide/porous carbon/silicon carbide aerogel composite for electromagnetic shielding prepared according to claim 1, wherein the composite is used as an electromagnetic shielding and wave absorbing material.
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